CN101747361A - Bridged polysilsesquioxane, monomer thereof and preparation method for two - Google Patents
Bridged polysilsesquioxane, monomer thereof and preparation method for two Download PDFInfo
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- CN101747361A CN101747361A CN200810239223A CN200810239223A CN101747361A CN 101747361 A CN101747361 A CN 101747361A CN 200810239223 A CN200810239223 A CN 200810239223A CN 200810239223 A CN200810239223 A CN 200810239223A CN 101747361 A CN101747361 A CN 101747361A
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- 239000000178 monomer Substances 0.000 title claims abstract description 69
- 229920000734 polysilsesquioxane polymer Polymers 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 20
- -1 ethoxy, methyl Chemical group 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910000077 silane Inorganic materials 0.000 claims abstract description 15
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 5
- 150000004985 diamines Chemical class 0.000 claims abstract description 5
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 150000003254 radicals Chemical class 0.000 claims description 6
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 150000005840 aryl radicals Chemical class 0.000 claims description 4
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 4
- 238000003980 solgel method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 239000000376 reactant Substances 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 125000003545 alkoxy group Chemical group 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 abstract 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 abstract 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 20
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 20
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 10
- 239000004593 Epoxy Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 235000019253 formic acid Nutrition 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 10
- 238000010792 warming Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 125000000962 organic group Chemical group 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 3
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000007818 Grignard reagent Substances 0.000 description 1
- 241001282153 Scopelogadus mizolepis Species 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000000304 alkynyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 150000004795 grignard reagents Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000001979 organolithium group Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
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Abstract
The invention discloses a bridged polysilsesquioxane, a monomer thereof and a preparation method for the two. The structural general formula of the monomer is as shown in Formula I, wherein in the structural general formula of the Formula I, R is a structure of Formula II or Formula III, and R1, R2 and R3 are selected from the following groups of methoxyl, ethoxy, methyl and phenyl; R' is C1-C10 aliphatic hydrocarbon, C4-C12 alicyclic hydrocarbon or C4-C12 aromatic hydrocarbon; and n is an integral number ranging from 0 to 10. The preparation method comprises the following step: in the inert atmosphere, making the silane monomer containing an epoxy group shown in the structural general formula of Formula IV react with the silane monomer containing amino shown in the structural general formula of Formula V or diamine shown in the structural general formula of Formula VI. The preparation method has the advantages of easy procuration of raw materials, simple synthetic method and moderate process and can prepare the bridged monomer with 6-12 alkoxy groups, the number of the alkoxy groups can be controlled by the selection of initial raw materials, and high product yield can be realized. H2N-R'-NH2 (Formula VI).
Description
Technical field
The present invention relates to bridging polysilsesquioxane field, particularly relate to a kind of bridging polysilsesquioxane and monomer whose and their preparation method.
Background technology
The bridging polysilsesquioxane is by comprising monomer that variable organic bridge linkage group and two or more trialkoxysilane groups the form hybrid inorganic-organic materials through the sol-gel technology preparation.The multiple key property that is arranged as organic field and inorganic field like this makes up and creates the brand-new synthetics with special performance special opportunity is provided.The diversity of molecule, the workability of adding gentle sol-gel condition and preparing sheet material, film, fiber etc. makes this class chemically stable and heat-staple material become the class critical material in the advanced material science and technology.
The diversity of this class material and many special performances all derive from the organic group of bridging, and these organic groups by Si-C with the form bond of covalent linkage on the trialkoxy silane polymkeric substance.The length of organic group, hardness, substituent geometrical dimension and functional group's degree all can change.Because organic bridge linkage group is the inherent integral part of hybrid material, so its variation just provides possibility for constructing such as overall performances such as porosity, thermostability, specific refractory power, optical property, chemical resistant properties, hydrophobic nature and specific inductivity, and does not exist than the threat that occurs on the big scale being separated.Flexible adjustability on material monolithic chemistry and the physical properties makes this type of material become the excellent candidate material that is fabricated onto support of the catalyst and ceramic precursor Application Areas from optics.
Preparation three kinds of a lot, the most frequently used methods of bridging monomer methods: the 1. metallization of aromatic base, alkyl, alkynyl presoma, and then with the silane reaction of four functionality; 2. the hydrosilylation of dienes (polyenoid class), or the diine class that is of little use, but 3. the organic group of two functionality reacts with the organic trialkyl silane that has reactive functionality.Method one needs to adopt Grignard reagent, organolithium or metal hydride that trialkoxy silane is handled, and makes the synthesis technique complexity, severe reaction conditions; Method two will adopt noble metal catalyst usually, waits the addition reaction of the Si-H group of trichlorosilane on the catalysis carbon-carbon double bond or trialkoxy silane as Platinic chloride, Karsted catalyzer.Method three is meant and can reacts with the organic molecule that has nucleophilic group that the bridging monomer that obtains by this method generally has only 6 alkoxyl groups when trialkoxy silane has an electrophilic group.
Summary of the invention
The purpose of this invention is to provide a kind of bridging polysilsesquioxane and monomer whose and their preparation method.
The monomer of bridging polysilsesquioxane provided by the invention, its general structure be suc as formula shown in the I,
(formula I)
(formula II) (formula III)
In the formula I general structure, R is the group shown in formula II or the formula III general structure, R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl and phenyl; R ' is the aliphatic group of C1-C10, the alicyclic hydrocarbon radical of C4-C12 or the aryl radical of C4-C12; N is the integer of 0-10.
The monomer methods of the above-mentioned bridging polysilsesquioxane of preparation provided by the invention, be in inert atmosphere, with the amino silane monomer that contains shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula V general structure, or react with the diamine shown in the formula VI general structure, obtain the monomer of the bridging polysilsesquioxane shown in the formula I general structure provided by the invention;
In the formula IV general structure, R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl and phenyl; N is the integer of 0-10;
In the formula V general structure, R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl and phenyl; N is the integer of 0-10;
In the formula VI general structure, R ' is the aliphatic group of C1-C10, the alicyclic hydrocarbon radical of C4-C12 or the aryl radical of C4-C12.
(formula IV)
(formula V)
H
2N-R′-NH
2
(formula VI)
In the aforesaid method, the mol ratio that contains amino silane monomer shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula V general structure is 1-4: 1, the monomeric mol ratio of diamine shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula VI general structure is 2-8: 1, the temperature of reaction of chemical reaction is 50-80 ℃, and the reaction times is 6-60 hour.
After above-mentioned reaction finishes, with the monomer of the bridging polysilsesquioxane that obtains under acid or alkaline condition, processing step according to conventional sol-gel method, comprise hydrolysis and condensation, gelation, ageing and drying step, this bridging monomer promptly changes highly cross-linked bridging polysilsesquioxane into.This bridging polysilsesquioxane and prepare the method for this bridging polysilsesquioxane also belongs to protection scope of the present invention.
The monomer methods of preparation bridging polysilsesquioxane provided by the invention, raw materials used being easy to obtains, and synthetic method is simple, the technology gentleness, can prepare the bridging monomer with 6-12 alkoxyl group, the number of alkoxyl group can be controlled by choosing of initial feed, the product yield height.
Description of drawings
The infrared spectrum of the bridging polysilsesquioxane that Fig. 1 prepares for embodiment 1.
The nmr spectrum of the bridging polysilsesquioxane that Fig. 2 prepares for embodiment 1.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.
Under nitrogen protection, 45ml 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane is joined condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 18ml 3-aminopropyl trimethoxysilane again, be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
9 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml tetrahydrofuran (THF), adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Infrared and the nmr spectrum of this compound respectively as depicted in figs. 1 and 2.As seen from the figure, the structure of this compound is correct.
Embodiment 2
Under nitrogen protection, 23ml 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane is joined condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 12ml 3-aminopropyl triethoxysilane again, be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
9 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml methyl alcohol, adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 3
Under nitrogen protection; with 43ml 3-(2; 3-epoxy third oxygen) the propyl group methyl dimethoxysilane joins condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 16ml 3-aminopropyl methyl dimethoxysilane again; be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
6 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml tetrahydrofuran (THF), adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 36 hours 50 ℃ of uncovered placements.
Embodiment 4
Under nitrogen protection; with 29ml 3-(2; 3-epoxy third oxygen) the propyl group methyl dimethoxysilane joins condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 12ml 3-aminopropyl trimethoxysilane again; be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
7 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml ethyl acetate, adding 1.2ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 5
Under nitrogen protection; with 55ml 3-(2; 3-epoxy third oxygen) propyl trimethoxy silicane joins condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 26ml 3-aminopropyl methyldiethoxysilane again; be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
8 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml ethanol, adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 6
Under nitrogen protection, 30ml 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane is joined condenser is housed, in the there-necked flask of thermometer and dropping funnel, add the 2.5ml quadrol again, be warming up to 50 ℃, react and obtain colourless bridging monomer after 6 hours.
12 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 20ml acetone, adding 0.2ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 7
Under nitrogen protection, 30ml 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane is joined condenser is housed; in the there-necked flask of thermometer and dropping funnel; add the 3.6g mphenylenediamine again, be warming up to 70 ℃, react the bridging monomer that obtains redness after 60 hours.
12 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 20ml tetrahydrofuran (THF), adding 0.2ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 8
Under nitrogen protection, 18ml 3-(2,3-epoxy third oxygen) propyl group methyldiethoxysilane is joined condenser is housed; in the there-necked flask of thermometer and dropping funnel; add the 10ml quadrol again, be warming up to 50 ℃, react and obtain colourless bridging monomer after 8 hours.
8 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml tetrahydrofuran (THF), adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 9
Under nitrogen protection, 35ml 3-(2,3-epoxy third oxygen) propyl group methyl dimethoxysilane is joined condenser is housed; in the there-necked flask of thermometer and dropping funnel, add 8g 4 again, the 4-diaminodiphenyl-methane; be warming up to 75 ℃, react and obtain brown bridging monomer after 48 hours.
8 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml tetrahydrofuran (THF), adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Embodiment 10
Under nitrogen protection; with 22ml 3-(2; 3-epoxy third oxygen) propyl-triethoxysilicane joins condenser is housed; in the there-necked flask of thermometer and dropping funnel; add 6.5ml 3-aminopropyl methyl dimethoxysilane again; be warming up to 70 ℃, react and obtain lurid bridging monomer after 48 hours.
8 tri-alkoxies are arranged in the resulting bridging monomer, get 5ml bridging monomer and be dissolved in the 10ml ethanol, adding 1ml mass percent concentration is 88% aqueous formic acid, can obtain the bridging polysilsesquioxane in 24 hours 50 ℃ of uncovered placements.
Claims (7)
1. the monomer of a bridging polysilsesquioxane, its general structure be suc as formula shown in the I,
(formula I)
In the described formula I general structure, R is the group shown in formula II or the formula III general structure;
(formula II) (formula III)
R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl, phenyl; R ' is the aliphatic group of C1-C10, the alicyclic hydrocarbon radical of C4-C12 or the aryl radical of C4-C12; N is the integer of 0-10.
2. a monomer methods for preparing the described bridging polysilsesquioxane of claim 1 is in inert atmosphere, and the amino silane monomer that contains shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula V general structure is reacted; Or the diamine shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula VI general structure reacted, obtain the monomer of the bridging polysilsesquioxane shown in the formula I general structure provided by the invention;
In the described formula IV general structure, R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl and phenyl; N is the integer of 0-10;
In the described formula V general structure, R
1, R
2And R
3All be selected from following radicals: methoxyl group, oxyethyl group, methyl and phenyl; N is the integer of 0-10;
In the described formula VI general structure, R ' is the aliphatic group of C1-C10, the alicyclic hydrocarbon radical of C4-C12 or the aryl radical of C4-C12.
(formula VI)
3. method according to claim 2 is characterized in that: the mol ratio that contains amino silane monomer shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula V general structure is 1-4: 1; The mol ratio of the diamine shown in silane monomer that contains epoxy group(ing) shown in the formula IV general structure and the formula VI general structure is 2-8: 1.
4. according to claim 2 or 3 described methods, it is characterized in that: described temperature of reaction is 50-80 ℃, and the reaction times is 6-60 hour.
5. according to claim 2 or 3 described methods, it is characterized in that: described inert atmosphere is nitrogen or argon gas atmosphere.
6. bridging polysilsesquioxane is with sol-gel method the monomer of bridging polysilsesquioxane to be prepared as reactant to obtain; It is characterized in that: the monomer of described bridging polysilsesquioxane is the monomer of the described bridging polysilsesquioxane of claim 1.
7. method for preparing the described bridging polysilsesquioxane of claim 6 is with sol-gel method the monomer of bridging polysilsesquioxane to be prepared as reactant to obtain; It is characterized in that: the monomer of described bridging polysilsesquioxane is the monomer of the described bridging polysilsesquioxane of claim 1.
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| CN102584886A (en) * | 2012-01-17 | 2012-07-18 | 华南理工大学 | Silane coupling agent and preparation method thereof |
| CN102603787A (en) * | 2012-02-14 | 2012-07-25 | 长安大学 | Synthesis method of monodisperse bridged polysilsesquioxanes microspheres |
| WO2012115769A2 (en) | 2011-02-25 | 2012-08-30 | Nalco Company | Reducing aluminosilicate scale in the bayer process |
| CN103319204A (en) * | 2013-06-05 | 2013-09-25 | 中国科学院上海硅酸盐研究所 | Application of bridged siloxane as pottery cultural relic reinforcing agent, and reinforcing method |
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| CN101220051A (en) * | 2007-12-29 | 2008-07-16 | 厦门大学 | Method for preparing double-octamer sesquialter siloxane with double-function substitutions |
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